TWI240015B - Electrostatic chuck member and method of producing the same - Google Patents
Electrostatic chuck member and method of producing the same Download PDFInfo
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- TWI240015B TWI240015B TW090101106A TW90101106A TWI240015B TW I240015 B TWI240015 B TW I240015B TW 090101106 A TW090101106 A TW 090101106A TW 90101106 A TW90101106 A TW 90101106A TW I240015 B TWI240015 B TW I240015B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/68—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for positioning, orientation or alignment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23Q—DETAILS, COMPONENTS, OR ACCESSORIES FOR MACHINE TOOLS, e.g. ARRANGEMENTS FOR COPYING OR CONTROLLING; MACHINE TOOLS IN GENERAL CHARACTERISED BY THE CONSTRUCTION OF PARTICULAR DETAILS OR COMPONENTS; COMBINATIONS OR ASSOCIATIONS OF METAL-WORKING MACHINES, NOT DIRECTED TO A PARTICULAR RESULT
- B23Q3/00—Devices holding, supporting, or positioning work or tools, of a kind normally removable from the machine
- B23Q3/15—Devices for holding work using magnetic or electric force acting directly on the work
- B23Q3/154—Stationary devices
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
- H01L21/6831—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using electrostatic chucks
- H01L21/6833—Details of electrostatic chucks
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- Computer Hardware Design (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Engineering (AREA)
- Container, Conveyance, Adherence, Positioning, Of Wafer (AREA)
- Jigs For Machine Tools (AREA)
- Manipulator (AREA)
- Coating By Spraying Or Casting (AREA)
Abstract
Description
1240015 五、發明說明(1) 【技術領域 本發明係有關於粒 件、絕緣性構件等吸電將導電性構件、半導體性構 造方法。 、疋所使用的靜電夾持構件及其製 【技術背景】 近來,基於自動化且防止 製造過程,W如半導髀制、生::、牛導體或液晶 . 體Ik表置之中’構成其一部分夕仏 真工或疋減壓的環境下進行。 由達成電路積集化或微細加工化的觀點看來,這種乾 式處理之中,有必要提昇矽晶圓或玻璃基板等之基板的^ 案化時的位置精確度。 以往’因應上述需求的方法例如,在基板搬移或吸附 固定時,使用了真空夾具或是機械性夾具。然而真空夾具 係在真空下處理,所以壓力差無法變大而使得吸附力弱, 即使能夠吸附,也僅能局部地吸附部分,而產生基板不正 的缺點。由於上述之晶圓處理的高溫化氣體無法冷卻,所 •以具有無法適用於最近高性能半導體製造程序之不便。另 一方面,使用機械式夾具時,由於裝置複雜,具有需要保 守檢查的時間的缺點。1240015 V. Description of the invention (1) [Technical Field] The present invention relates to a method for constructing conductive members and semiconductors by absorbing electricity such as pellets and insulating members. The electrostatic clamping member and its manufacturing technology background [Technical background] Recently, based on automation and prevent manufacturing process, such as semi-conductor fabrication, production :, cattle conductor or liquid crystal. In the body Ik table, 'constitute its Part of the work is carried out under real working conditions or under reduced pressure. From the standpoint of achieving circuit accumulation or microfabrication, it is necessary to improve the position accuracy of a silicon wafer or a glass substrate such as a substrate during the dry processing. Conventionally, a method that responds to the above-mentioned needs, for example, a vacuum jig or a mechanical jig is used when a substrate is moved or fixed by suction. However, the vacuum clamp is processed under vacuum, so the pressure difference cannot be increased to make the adsorption force weak, and even if it can be adsorbed, it can only partially adsorb the part, resulting in the disadvantage that the substrate is not correct. Since the above-mentioned wafer processing high-temperature gas cannot be cooled, it has the inconvenience that it cannot be applied to the recent high-performance semiconductor manufacturing process. On the other hand, when a mechanical jig is used, there is a disadvantage that the inspection time is required due to the complexity of the device.
2053-3738-PF.ptd 最近,為了改善如上所述的習知技術,利用靜電力的 靜電夾具被開發並且廣泛地使用。然而此技術亦有以下的 問題點。2053-3738-PF.ptd Recently, in order to improve the conventional technique as described above, an electrostatic clamp using electrostatic force has been developed and widely used. However, this technique also has the following problems.
第4胃 1240015 五、發明說明(2) 此為’使用靜電夾具吸附 而具有基板無法卸下的 壓之後,基板與靜電夾具之間=基板時’在切斷施加電 所以具有若無法完全地去除電荷了電何(吸附力作用), 問題點。 上述對策,習知,在該耩φ + θ 的改良。例如: #電夹具使用絕緣性介電材質 示了使用氮化鋁與氮化 當作高絕緣物的例子。 揭示了在高絕緣物的表 ,並且與Si + SiC板的例__ 特開平6 -80 89號公報之中,揭 欽粉末的混合物之燒結體或溶射膜 特開平6 - 3 0 2 6 7 7號公報之中, 面塗覆氧化鈦之後,在上方塗覆|呂 子。 } 特公平6-36583歡公報之中,揭示了使用氧化鋁以當 作絕緣性體的例子。 特開平5 -23 5 1 52號公報以及特開平6 —8〇89號公報之 中’揭示了使用氧化鋁、氮化鋁、氧化鋅、氮化硼、矽, 铭,氮化合物等當作高絕緣體的例子。 特開平3 -1 4 7 8 4 3號公報以及特開平3 - 2 0 4 9 2 4號公報之 中’揭示了有必要使用更大的靜電力時,在高絕緣體添加 介電率高的Ti02而降低體積固有阻抗率以提昇靜電力的方 法。 含有Ti〇2的八12 03等高絕緣體,在電源OFF時,有殘留 暫時的時間吸附力之缺點。在此,克服此缺點的技術例 f ’特開平1 1 - 2 2 2 8 2 6號公報或特開平1 1 - 6 9 8 5 5號公報 等’為了縮短矽晶圓的脫離時間,揭示了反轉電極極性的The fourth stomach 1240015 V. Description of the invention (2) This is 'After the substrate is held by an electrostatic clamp and the pressure cannot be removed, the substrate and the electrostatic clamp = when the substrate is used' When the power is cut off, it cannot be completely removed. What is the charge (adsorption), the problem. The above countermeasures are known to be improved in this φφ + θ. For example: #Electric fixture uses insulating dielectric material. It shows an example of using aluminum nitride and nitride as high insulators. An example of a high-insulator sheet and Si + SiC plate is disclosed in JP-A-6-80 89, a sintered body or a spray film of a mixture of powders disclosed by JP-A-6- 3 0 2 6 7 In the No. 7 bulletin, after the surface is coated with titanium oxide, it is coated thereon. } In Japanese Patent Publication No. 6-36583, an example of using alumina as an insulator is disclosed. Japanese Unexamined Patent Publication No. 5-23-23 5 52 and Japanese Unexamined Patent Publication No. 6-8089 disclose the use of aluminum oxide, aluminum nitride, zinc oxide, boron nitride, silicon, silicon nitride, and nitrogen compounds. Examples of insulators. Japanese Patent Application Laid-Open No. 3 -1 4 7 8 4 3 and Japanese Patent Application Laid-Open No. 3-2 0 4 9 2 4 disclose that when a larger electrostatic force is necessary, Ti02 with a high dielectric constant is added to a high insulator. And the method of reducing the volume intrinsic resistivity to increase the electrostatic force. The high-insulation insulators such as TiO2 and TiO2 have the shortcoming of a temporary adsorption force when the power is turned off. Here, a technical example f 'which overcomes this disadvantage is disclosed in JP-A No. 1-2 2 2 8 2 6 or JP-A No. 1-6 9 8 5 5 etc., in order to shorten the silicon wafer detachment time. Reversing electrode polarity
1240015 五、發明說明(3) 方法。 圓 法 中 f開平"4663Λ公報之中’為了迅速地脫離石夕曰曰 揭不了在絕緣層的-部分塗覆具有導電性的形成曰方 低的情形,揭示了具有水冷構造之靜電::=的“降 因此,使用靜電夾具之A 1? 〇, · τ彳η相λα — 層,具有以下的問題: "Tl〇2類的南絕緣性溶射 (1)混合有Ti〇20nl2〇3類的熔射層,體積固有阻抗彳 二並且小的電流,所以可預期因強森拉貝克效應 (A· JensenM.Rahbek’s f0rce)而提昇靜電力。缺而,1240015 V. Description of the invention (3) Method. In the f Kaiping " 4663Λ bulletin of the circle method, in order to quickly get rid of Shi Xiyue, it is impossible to expose the case where the-part of the insulating layer is coated with conductivity to form a low square, revealing static electricity with a water-cooled structure :: = "Due to this, using the A 1? 〇, · τ 彳 η phase λα — layer of the electrostatic fixture, has the following problems: " Tl02-type south insulating spray (1) mixed with Ti〇20nl203 This type of spray layer has a volume intrinsic impedance of 22 and a small current, so it can be expected that the electrostatic force will be enhanced by the Jensen M. Rahbek's f0rce effect.
TiOJ半導體物質,所以電荷的移動速度慢,所以停止電 ΐ 的應答特性(飽和吸附加到達時間、吸附力消滅 時間)變差,並且此特性特別在低溫環境更加顯著。 再者,為了使體積固有阻抗變成實用狀態之1χ 1〇9 Ω · cm,也必須混合Ti〇2於25衬%左右。但是,半導體製 造程序之中,添加多量的Ti〇2,意謂著混入不純物,此會 導致,質的降低,同時為污染作業環境的原因。 及附的半導體晶圓在室溫以上時,由於體積固有阻抗 過低’所以流動大的漏電流而破壞晶圓電路的可能性高。 / ,=)混合有Ti〇2的αι2 03類的熔射層係藉由熔射法進 行…、:而’此方法所得到的該被覆層之體積固有阻抗以及 吸附力的偏差變大,生產性變低,所以成為成本提高的原The TiOJ semiconductor material has a slow charge moving speed, so the response characteristics (saturation adsorption plus arrival time, adsorption force elimination time) of the stoppage of the electrons are deteriorated, and this characteristic is particularly significant in low temperature environments. In addition, in order to make the volume intrinsic impedance into a practical state of 1 × 109 Ω · cm, it is also necessary to mix Ti02 with about 25% by weight. However, the addition of a large amount of Ti02 to the semiconductor manufacturing process means that impurities are mixed in, which will cause a reduction in quality and cause pollution to the working environment. When the attached semiconductor wafer is at room temperature or higher, the volume inherent resistance is too low, so a large leakage current may flow and damage the wafer circuit. / , =) Α 2 02 type spraying layer mixed with Ti〇2 is carried out by the spraying method ..., and 'the deviation of the inherent volume resistance and adsorption force of the coating layer obtained by this method becomes large, and production The performance becomes lower, so it becomes the cause of cost increase.
Η^ιιι麵 第6頁 1240015Η ^ ιι 面面 Page 6 1240015
因此, 並且減少其 本發明 止電壓施加 本發明 膜,因為與 中所含之鹵 污染環境之 本發明 絕緣基板, 出克服此的 本發明 件在金屬製 緣層,含有 的生產性與 性。 【發明 本發明 金屬質電極 陶瓷構成的 亦即, 至少一個表 物上具有Al9 此發明的 偏差,且 品質佳的靜電 在於,提供吸 時的應答性能(釋放)佳 另一目的在於,提供靜 觸的電漿等物 學性侵蝕作用 另一目的 矽晶圓接 化物之化 虞的Ti〇2 另一目的在於,針對以 度變化時有容 在使用溫 替代方案。 還有另一目的在於,為 圍以陶瓷構成 由熔射法形成 覆密著性,使 電極的周 電極而藉 良好的塗 夾持構件。 机 力強、另-方面停 的諍電失持構件。τ 電失持構件用熔射塗 理性侵餘作用或是環J 的損傷,並且不使用; 燒結法製造之習知A1 0 易損壞的缺點,所以2“’· 了克服習知靜電夾持構 溶射層之缺點,不僅絕 其大部分,並且具有高 其發揮良好的靜電特 之揭示】 之靜電夾持構件不僅於金屬製基板的表面形成 ’亦藉由熔射方式堆疊形成電阻率大之氧化物 絕緣層。 本發明靜電夾持構件基本的構造為,基材上的 面具有金屬質的底部塗覆物,並且此底部塗覆 03陶瓷構成的下部絕緣層,再者,此下部絕緣Therefore, the present invention reduces the application of the voltage-stopping film of the present invention, because the insulating substrate of the present invention which pollutes the environment with the halogen contained in the present invention, the present invention overcomes this by including the productivity and performance of the metal edge layer. [Invention of the metal electrode ceramic of the present invention, that is, at least one surface has the deviation of Al9 according to the present invention, and the high-quality static electricity is to provide a good response performance (release) during suction. Another purpose is to provide static contact. The physical erosion of plasma and other materials, Ti02, which is another purpose of silicon wafers, is another purpose, and it is aimed at allowing temperature to be used when the temperature changes. Still another object is to coat the member with a good coating so as to surround the electrode with a ceramic coating formed by a spray method. An electroenergetic miscarriage with strong power and another stop. τ The electrical runaway member is spray-coated with rational backlash or damage to ring J, and is not used; the conventional method of sintering A1 0 is easy to damage, so 2 "'· overcomes the conventional electrostatic clamping structure The shortcomings of the spray-emitting layer are not only most of them, but also have high electrostatic characteristics. The electrostatic clamping member is not only formed on the surface of the metal substrate, but also is formed by stacking by spraying. The basic structure of the electrostatic clamping member of the present invention is that the surface on the substrate has a metallic bottom coating, and this bottom is coated with a lower insulating layer made of 03 ceramic, and the lower insulating
1240015 五、發明說明(5) 】2有金屬質電極層,並 m緣層以當作頂部塗覆物“ί 構 的熔射層,其次屬二 下°卩絕緣層為厚度100〜500 層,並且此金屬f冑極/電/^層人為厚—度5〜100心的溶射 率最好為卜7%。、 曰虱虱含有量為2wt%以下,氣孔 A 12 〇3陶究構成之上邱紹接成 ^ ^98. 〇wt% a j, ^ ^ #/ΛΤΛΥ ^ ^ ^ ^ ^ 最好形成為1〜8%。 材枓如末熔射而成,並且氣孔率 上述上部絕緣層以Β Τ 由浸潰有機系或無機系的石夕;=層至少一者的表面’藉 此層的體積固體阻抗率;c進行封孔處理,並且 範圍。 机早最好介於lx 1〇13〜IX 1〇ΐ5Ω .⑽的1240015 V. Description of the invention (5)] 2 has a metal electrode layer, and the m-edge layer is used as a top coating of the "spraying layer" structure, followed by two degrees. The insulation layer is 100 ~ 500 layers thick. In addition, the metal f 胄 pole / electricity / thickness layer is artificially thick—the degree of emissivity is preferably 7%. The content of lice is less than 2wt%, and the stoma A 12 〇3 is based on the structure Qiu Shaocheng ^ ^ 98. 〇wt% aj, ^ ^ # / ΛΤΛΥ ^ ^ ^ ^ ^ It is best to form 1 ~ 8%. The material is formed by thermal spraying, and the porosity of the upper insulating layer is B. Τ is composed of impregnated organic or inorganic rocks; = the surface of at least one of the layers' takes the volume solid resistivity of this layer; c performs sealing treatment, and the range. The machine early is preferably between lx 1〇13 ~ IX 1〇ΐ5Ω.⑽
Ni 以 ίϊϋ極層最f 為選自 W、A1、Cu、Nb、Ta、Μ。、 形成的層。M上坆些金屬70素的合金之中至少1種熔射 ‘昇兩ί:ίΑ」2,陶究J成的下部絕緣層之間,具有用來提 5 ί' Μ ΐΐ質底部塗覆物,其最好選自Ni、 A1 Cr、Co、Mo以及含有1籍1V u、丄 中1種以上熔射形成。 上思些金屬元素的合金之 位於本發明靜電夾持構件 部絕緣層之頂部塗覆物,層之叫陶曼構成的上 在此接觸面施以機械加工石f晶圓的接觸面’最好 M i成表面粗度大約 1240015 五、發明說明Ni is selected from W, A1, Cu, Nb, Ta, and M based on the electrode f. , The formed layer. Among the alloys of 70 metals on M, at least one of the two kinds of molten shots is raised: ίΑ ″ 2, between the lower insulating layer of Tao JJ, with a bottom coating for improving 5 Μ ΐΐ It is preferably selected from the group consisting of Ni, A1 Cr, Co, Mo, and one or more types of 1V u and ytterbium. It is considered that the coating on the top of the insulating layer of the electrostatic clamping member part of the alloy of the metal element is called the contact surface of the layer called "Taumann", and the contact surface on which the machining surface is processed is preferably The surface roughness of M i is about 1240015. 5. Description of the invention
Ra:0. 1〜2. 〇 左右。 金屬質底部ί構件的製造之溶射法例如, 法等也ΐ以,!浆溶身?、減壓電漿溶射法、爆發炫射 用大氣f方面丨2 〇3陶瓷絕緣塗覆膜的施工可採 =電漿熔射法、減M電聚熔 【圖,之簡單說明】 寻 【實概念性地顯示本發明的靜電央具的剖面構造。Ra: 0. 1 ~ 2. 〇 or so. For example, the metal-bottomed member is manufactured by the solvent injection method, such as the method. Pulp melted? , Reduced pressure plasma dissolution method, explosive f atmosphere 丨 2 〇3 ceramic insulation coating construction can be mined = plasma spray method, M-reduction electrofusion melting [picture, a simple explanation] find [actual The cross-sectional structure of the electrostatic luminaire of this invention is shown conceptually.
【貫轭發明的最佳形態】 j囬偁W 加以說明。針對利用溶射法製造本發明之靜電夾具的例子籲1< 首先’將金屬製基材的裘而& 屬質_料加以熔射金 成底部塗覆物(under coat)。藉c材表面形 上形成Al2〇3陶竟構成的下部熔射絕:η其底部塗覆物 熔射法在下部熔射絕緣層的表:、邑然採用 形成t屬質溶射電極層,使得可藉此ϊ:ΐ; 述金屬質熔射電極声上, 電極。接耆在上 ‘絕緣層。藉此,製:如第日所_、 l2〇3陶瓷,以形成熔射 持構件。 圖所不具有積層構造之靜電夾 屬質層= : = 從 樣的使用環境,也不會受到環境中 影響’並且經過長時間,亦可永久維持初電浆的 2053-3738-PF.ptd 第9頁 1240015 五、發明說明(7) 比起Al2〇3陶瓷上部· 熔射電極層的直徑最好使用;少:二的直經’上述金屬質 由為,不露出電極的端面於外部。 上的物質。其理 之中,符號1為金屬製基板,2A金屬暂 熔射層構成的底部塗覆物,3為板2為金屬質 熔射絕緣層,4為金屬質熔射電極声,2 3陶竞構成的下部 =射?陶竞之上部溶射絕緣層曰為頂二 電源,8為接地,9電磨負荷用的銅線。巧夕曰曰困,7為直流 10為上部熔射絕緣層3與下部熔射絕 — 的符號 熔射絕緣層直接接觸的位置。、、’ B 母個A丨2〇3陶瓷 料,=传=形f上述金屬質底部塗覆物2的溶射材_ 料最好使用Nl、Al、Cr、Co、Mo等金屬式曰從、 些金屬的合金,層厚产為30〜ϋχ 3疋種以上這 權厚度馮川300#m,最好為50〜150"m 2疋因為,層厚度小於30,的話,具有層厚度不平。 缺點’另一方面,層厚度大於30 0 //m以當作勺、 j,在機能上不會特別地提昇,所以從經 = 考量,並不恰當。 系上的 形成於底部塗佈層2,且位於金屬質之溶射電極芦 €· 上部、下部,而夾層地形成的ΜΑ陶瓷構成的上部θ傾 緣層、下部熔射絕緣層,被要求有良好的電氣絕緣性、耐 腐蝕性、耐電漿腐蝕性。因為此層必須純度高且緻密。發 明者們藉由實驗確認,了解到純度9 8%以上,尤其是“。今 上的話,熔射塗覆層的氣孔率為卜8%、尤其是^以 圍。 呵軏[The best form of the yoke invention] J 回 jW will be described. With regard to an example of manufacturing the electrostatic jig of the present invention by a solvent injection method, < First, ' a metal substrate made of a metal substrate is spray-molded with gold to form an under coat. By using the surface of c material to form the lower part of Al2O3 ceramics, the following shot: η its bottom coating shot method on the surface of the lower shot insulation layer :, Ran uses the formation of the t-type plasma solvent electrode layer, so that This can be used: ΐ: 金属 The metal melting shot electrode, the electrode. ‘Insulation.’ By this, the system is made as in the first day, ceramics to form a shot holding member. As shown in the figure, the electrostatic clip is not a laminated layer =: = From the use environment, it will not be affected by the environment ', and after a long time, it can also permanently maintain the initial plasma of 2053-3738-PF.ptd Page 9 1240015 V. Description of the invention (7) Compared with the upper part of Al2O3 ceramics, the diameter of the spray electrode layer is best used; less: two straight through the above-mentioned metal, so that the end face of the electrode is not exposed to the outside. On the substance. Among them, the symbol 1 is a metal substrate, 2A is a bottom coating composed of a temporary metal spray layer, 3 is a plate 2 is a metal thermal spray insulation layer, 4 is a metal thermal spray electrode sound, 2 3 Tao Jing The lower part of the composition = shoot? The upper part of Tao Jing's dissolving and radiating insulation layer is called the top two power source, 8 is the ground wire, and 9 is the copper wire for electric grinding load. Qiao Xi said sleepy, 7 is the direct current 10 is the symbol of the upper thermal spray insulation layer 3 and the lower thermal spray insulation — the position where the thermal spray insulation layer directly contacts. , 'B female A 丨 203 ceramic material, = pass = shape f the above-mentioned metal base coating 2 of the molten shot material _ material is best to use Nl, Al, Cr, Co, Mo and other metal formulas, such as, For some alloys of these metals, the layer thickness is 30 ~ ϋχ 3 疋. This thickness is 300 # m, preferably 50 ~ 150 " m 2m, because if the layer thickness is less than 30, the layer thickness will be uneven. Disadvantage ’On the other hand, the thickness of the layer is greater than 30 0 // m to be used as a spoon, j, and it will not be particularly improved in function, so it is not appropriate to consider from the classics. It is formed on the bottom coating layer 2 and is located on the upper part and lower part of the metal spray electrode. The upper θ bevel layer and the lower shot insulation layer composed of Μ ceramics formed in a sandwich are required to be good. Electrical insulation, corrosion resistance, plasma corrosion resistance. Because this layer must be high purity and dense. The inventors confirmed through experiments that the purity was more than 98%, especially ". Nowadays, the porosity of the spray coating layer is 8%, especially around ^. Hehe
2053-3738-PF.ptd 1240015 五、發明說明(8) 形成於下部熔射絕绫 好熔射選自w、A丨r、1τι;表面的金屬質熔射電極層,最 屬至少一種的金屬而形成者、〇、Nl以及各有這些金 Am的範圍。1理由 再者,其厚度最好在5〜100 當作電極之作用機能會降;f。度若小於5 =層的多孔質 別是,10〜30㈣較適ς有特別地提昇,所以不經濟。特 的氣Ϊ : :1 層:=工雖=愈小愈好,然而以熔射法形成 題。並且,Ρ , 經過實驗證實沒有特別的問 疋上述氣孔率為1%以下的話,在大氣中熔射__ 環境氣體中的腐餘::合;mL率大於?%的話’在 羊增同而發熱’並使得電極層高溫化,所以不適合。 瞪盔5熔f電極層’使金屬在大氣中熔射時所產生的氧化 5電阻來源’此並非所希望的。藉由實驗結果,已確認 =1有2%以下的混入量,以當作溶射電極層,沒有特別的 員壞所以本發明所形成的熔射電極層具有2 %以下的氧含 有量。 、其次’形成於最上層以當作頂部塗覆物之A 12〇3陶究構 成的上部熔射絕緣層,最好利用機械加工(研削)將其表面__ 研削成與金屬製基板表面平行,並且完成表面粗度Ra為〇 卜0 · 2 // Μ以下。 · 特別是,可視需要,在此機械研削過的上部熔射絕緣 層,塗佈液體有機矽化合物(曱基·甲矽烷·三·異氰酸2053-3738-PF.ptd 1240015 V. Description of the invention (8) The thermal spray formed on the lower part must be selected from w, A 丨 r, 1τι; the metallic spray electrode layer on the surface, which is at least one kind of metal The former, 0, Nl, and each of these gold Am ranges. 1 Reasons Further, the thickness is preferably in the range of 5 to 100, as the function of the electrode will be reduced; f. If the degree is less than 5 = porous of the layer, in particular, 10 to 30% is more suitable, and it is particularly uneconomical. Special discouragement:: 1 layer: = work though = the smaller the better, but the problem is formed by the spray method. In addition, it has been confirmed through experiments that if the porosity is less than 1%, it will be sprayed in the atmosphere __ residues in the ambient gas :: together; if the mL rate is greater than?% It is not suitable because it generates heat and heats up the electrode layer. The glaze helmet 5 melts the f-electrode layer, which is a source of oxidation generated when the metal is sprayed in the atmosphere. This is not desirable. According to the experimental results, it has been confirmed that = 1 has a mixing amount of 2% or less, and it is used as a dissolution electrode layer. There is no special damage. Therefore, the sputter electrode layer formed by the present invention has an oxygen content of 2% or less. Secondly, the upper layer of A 12 03 formed by the top layer of A 1203 ceramics is used as a top coating. It is best to use machining (grinding) to grind the surface __ parallel to the surface of the metal substrate , And the completed surface roughness Ra is 0 0 0 2 / M or less. · In particular, if necessary, apply a liquid organic silicon compound (fluorenyl · silane · tri · isocyanate) to the upper shot-blasted insulating layer ground by this machine.
2053-3738-PF.ptd 12400152053-3738-PF.ptd 1240015
五、發明說明(9) 鹽;苯基·甲矽烷·三·異氰酸鹽或是無機矽化合物(珍醇 鹽;鹼金屬之矽化合物),然後在1 2 0〜3 5 0 °C加熱1〜5小時,° 加以封孔處理。此封孔處理精由殘存於炼射層中的微細1 孔部填充矽化合物,可防止異物的附著,並且可防止作g 環境中的腐#氣體的侵入。並且,此封孔處理,也可以豐j 下部的A 12 〇3陶究溶射絕緣層進行。 如以上所說明,金屬質熔射層的底部塗覆物、金屬質 溶射電極層、A丨2〇3陶瓷構成的上部·下部熔射絕緣層的施 工可使用電漿熔射法、高速火燄法、爆發熔射法、^光^ 射法(僅金屬質),然而由生產性、品質安定性的觀點看' 來’特別是大氣電漿熔射法或減壓電漿熔射法較為合、商。 實施例1 ^ 在紹基材(寬度50mmx長度lOOmmx高度5mm)的部分施 以喷砂處理以粗面化之後,利用火談炫射法處理 «· 80wt%Ni-20wt%Al合金,以在此粗化處理面上,形成厚度 8 0 β m之底部塗覆物。然後,利用大氣電漿熔射法在上述 底部塗覆物上形成厚度1 5 〇 // m的A丨2 〇3陶瓷,接著,利用大 氣電漿熔射法在A丨2〇3陶瓷熔射層上形成6〇 的金屬鶴 W),以當作熔射電極層。並且,此時電極層中的氧量為 〇·11 wt%。其次,利用大氣電漿熔射法在上述金屬鎢電極 層的表面積層形成厚度3〇 Am〜5〇〇 //111的人丨2〇3陶瓷之上部熔 射絕緣層’以當作頂部塗覆物,然後當作試驗片。 將如上所製作的試驗片,放置於以下之腐姓性環境下 連續20 0個小時,以調查因侵〜A12〇3陶瓷構成之上部、馆^射V. Description of the invention (9) Salt; phenyl · silane · tri · isocyanate or inorganic silicon compound (zhenolate; silicon compound of alkali metal), and then heating at 1 2 0 ~ 3 5 0 ° C 1 to 5 hours, ° Sealing treatment. This sealing treatment essence is filled with a silicon compound remaining in the fine 1-hole portion of the refining layer, which can prevent the adhesion of foreign substances and prevent the intrusion of rot gas in the environment. In addition, this plugging treatment can also be performed with A 12 〇 3 ceramic solvent-sprayed insulating layer in the lower part of Feng j. As described above, the construction of the bottom coating of the metal spray layer, the metal spray electrode layer, and the upper and lower thermal spray insulation layers made of A203 ceramic can be performed by plasma spray method or high-speed flame method. , Burst spray method, ^ light ^ spray method (only metallic), but from the viewpoint of productivity and quality stability, 'come', especially atmospheric plasma spray method or decompression plasma spray method are more suitable, Business. Example 1 ^ After sandblasting the part of the base material (width 50mmx length 100mmx height 5mm) to roughen it, the flame method was used to treat «· 80wt% Ni-20wt% Al alloy, here On the roughened surface, a bottom coating having a thickness of 80 β m was formed. Then, an atmospheric plasma spraying method was used to form A 丨 2 03 ceramics with a thickness of 1 5 0 // m on the bottom coating. Then, an atmospheric plasma spraying method was used to spray A 丨 203 ceramics. A metal crane (60) was formed on the layer to serve as a thermal spray electrode layer. In this case, the amount of oxygen in the electrode layer was 0.11 wt%. Next, an atmospheric plasma spray method is used to form a thickness of 30 Am ~ 500 // 111 on the surface area layer of the above-mentioned metal tungsten electrode layer. The upper part of the 203 ceramic is a thermal spray insulation layer to be used as a top coating And then used as a test strip. The test piece produced as described above was placed in the following rotten environment for 200 consecutive hours to investigate the invasion of ~ A1203 ceramics, including the upper part and the hall.
No. 1240015 五、發明說明(ίο) 絕緣層的氣孔部之腐触成份,導致金屬鎢電極之腐触發生 狀況。 (1 )鹽水喷霧試驗(JIS Z 23 71 ) (2)耐鹵素腐蝕試驗(將試驗片靜置於,導人每分鐘 120ml之CHF3 4 0ml+Ar 60ml混合氣體於塑膠製腐钱試驗 裝置的環境中,試驗溫度為60 °C ) " 上述腐蝕性試驗結果如表1簡要地顯示。如表丨所示的 結果,ai2o3陶瓷構成之上部熔射絕緣層的厚度為8“m以 上的話’在進行鹽水喷霧試驗'耐南素腐餘試本身,可遮 斷侵入内部的腐蝕性成份,並且鎢雷 > 办赢· Μ认外几二输处 1且瑪電極層完全被認定無腐籲馨 4uh 说07外規0相對於此,Al2〇3陶 瓷構成之上部熔射絕緣層的厚度若炎 腐钱性成份通過氣孔部而入二30 口的話’ 而出現電極機能消失的傾向:€件鶴電極層嚴重腐姓’ 表 表面的構造 耐腐钱試驗No. 1240015 V. Description of the Invention (ίο) The corrosion component of the pores of the insulating layer causes the corrosion of the metal tungsten electrode. (1) Salt water spray test (JIS Z 23 71) (2) Halogen corrosion resistance test (Place the test piece in a static state, and introduce a mixed gas of 120 ml of CHF3 40 ml + Ar 60 ml per minute into a plastic corrosion test device. In the environment, the test temperature is 60 ° C) " The results of the above corrosive test are shown in Table 1 briefly. As shown in Table 丨, if the thickness of the upper layer of the spray insulation layer made of ai2o3 ceramic is 8 "m or more, the salt spray resistance test will be performed during the salt spray resistance test, which can block the corrosive components invading the interior. And Tungsten Thunder &Win; M wins the first two losses and the M electrode layer is completely determined to be non-corrosive. 4Uh said that 07 external regulations 0. On the other hand, Al2O3 ceramics constitute the upper part of the spray insulation layer. If the thickness of the hot and corrosive ingredients enters the second 30 mouths through the stomata, the electrode function tends to disappear: a piece of crane electrode layer is severely corrupted.
(備註)··(〇層厚度單位為V 腐钱變55££a 無異tZZZsgt m 耐鹵素蝕刻 試驗 廣飯變色大 塵飯變色大 無異常 無異常 i異常 備註 比較例 發明例 2053-3738-PF.ptd 第13頁 1240015(Remarks) ... (0-thickness unit is V. Corrosion change 55 ££ a no difference tZZZsgt m halogen resistance test wide rice discoloration large rice discoloration large dust rice discoloration no abnormality no abnormality i abnormal note Comparative Example Invention Example 2053-3738- PF.ptd Page 13 1240015
(2)腐蝕試驗後的試驗 部絕緣層,而露出電極表面,’僅以機械式方式去除上 接觸的上部絕緣層的變色悴^二且以其外觀變化以及與i 旧况來評價。 、 實施例2 本實施例之靜電夾持 6-36583號)等提案的金屬 熱衝擊性試驗。 =件與先行技術(例如特開平 電極之四周的熔射形成物之耐 (1)本發明使用於靜電夾持構件之層構造 使用大氣電漿熔射法與減壓電漿熔射法以 龍厚度、製基材之_面, 2 , 以大氣電漿熔射法形成丨5 〇 # m的 ② 下部熔射絕緣層99· 5wt% 之Al2〇3 〇 ③ 金屬質電極層: a b ④上部熔射絕緣層 99. 5wt% 之Al2〇3 〇 (2 )比較例的構造 以大氣電漿熔射法形成30 的 金屬W 以減壓電漿熔射法形成30 的 金屬W 以大氣電漿熔射法形成150 //m的 ①底部塗覆物:a·以大氣電漿熔射法形成厚度丨〇〇的80wt%Ni-20wt%Al(2) After the corrosion test, the insulating layer of the test portion is exposed, and the electrode surface is exposed, and only the discoloration of the upper insulating layer in contact with the upper part is removed mechanically, and the appearance change and the old condition are evaluated. 2. Example 2 Electrostatic clamping No. 6-36583 of this example) Proposed metal thermal shock test. = Parts and prior technology (such as the resistance of the spray formation around the kaiping electrode) (1) The present invention is used for the layer structure of the electrostatic clamping member. The atmospheric plasma spray method and the reduced-pressure plasma spray method are used to The thickness and the thickness of the substrate, 2 are formed by atmospheric plasma spraying method. 5 〇 # m of ② the lower shot insulation layer 99 · 5wt% of Al 2 0 3 ③ metal electrode layer: ab ④ upper melting The structure of the comparative example of Al 2 O 3 〇 (2) with an insulating layer of 99.5 wt% was formed by forming a metal W of 30 by an atmospheric plasma spray method and forming a metal W of 30 by a reduced-pressure plasma spray method. Forming 150 // m ① bottom coating: a · 80wt% Ni-20wt% Al with a thickness of 丨 〇〇 formed by atmospheric plasma spray method
2053-3738-PF.ptd 第14頁 1240015 — 五、發明說明(12) ②絕緣層:以大」=覆物 99.5wt%iAl2〇3。乳電水熔射法形成厚度15〇 "««的 e u ,比較例係對直徑為10〇nm、厚产為贺 基材的整個周圍塗覆。 序戾馮lUmm的AI良 (3 )熱衝擊試驗條彳 在空氣中35〇0Cy 4 g y, 氣吹!。分鐘的操作告作力;’以25。。的壓縮空 驗。 田作1 一人循鞦,而貫施1 0次循環的試 ·· (4)试驗結果 上述試驗的結果顯示於表2。從 知,圍繞著㉟製基材周圍之熔射之比較例付 底部塗覆物,經過1〜3次循淨德合甚 ' _有…、 為,在义灸曰產生龜裂。此原因應該 ΐ,ΐ曰ίί 2 3溶射層的熱膨脹率大大地不同的方 ’因為形成圍繞著基材周圍的層,所UI g „ 極大的應力的結果。 所以在此層負何 環之用於本發明構造要件的層為經過w次循 ^。㈣維持元整狀態,並以能夠發揮高耐熱衝擊性的2053-3738-PF.ptd Page 14 1240015 — V. Description of the invention (12) ② Insulation layer: Large ”= covering 99.5wt% iAl203. The emulsion galvanophoresis method was used to form e u with a thickness of 15 °, and a comparative example was applied to the entire periphery of a substrate having a diameter of 100 nm and a thick substrate. Xu Yi Feng Feng AImm (3) Thermal shock test strips: 3500Cy 4 g y in air, air blow !. Minutes of operation are working; 'Take 25. . Compression test. Tian Zuo 1 performed the test by himself and performed 10 cycles. (4) Test results The results of the above tests are shown in Table 2. It is known that the comparative example of the thermal spray around the base material is coated with the bottom coating, and after 1 to 3 cycles, it is clear that there is a crack in the moxibustion. The reason for this should be: “The thermal expansion coefficient of the 2 3 lysing layer is greatly different.” Because the layer surrounding the substrate is formed, the UI g „is the result of great stress. So what is the role of this layer? The layer required for the structural elements of the present invention has been subjected to w cycles ^. ㈣ maintains the unitary state, and has a high thermal shock resistance
1240015 五、發明說明(13) 表2 表面ί mi ~~ 熱衝擊條件 No. 底部塗 覆物 下部絕 缘層 金屬電 極層 上部絕 綠層 350〇CX 15 分鐘 <=>空氣冷卻 備註 1 有 有 有*0) 有 10次循環後亦無異常 比較例 2 有 有 有 *(2) 有 10次循環後亦無異常 3 有 無 無 有 3次循環後亦無異常 4 無 無 無 有 次循環後亦無異常 發明例 (備注)(1)底部塗覆物為厚度100//m的8〇wt%Ni—2〇wt%A1 (2) 金屬電極層*(1)為以大氣電漿熔射法形成3〇 的金屬w(氧含量為〇·丨2^^參 *(2)為以減壓電漿熔射法形成3〇 r, . ^ ^ ^ 的金屬W(氧含量為0.12wt%) (3) 絕緣層為上下皆使用a 1 〇 。+丄^ Γ白1史用Ai2〇3之大氣熔射法150 β m 實施例3 本實施例係將矽晶圓吸附於靜電夾持 將電源OFF時的殘留吸附力隨著時間的變化再仟之後,測试 (1)在適合於本發明的條件下製造的靜 構成的直徑6彳的A i基材上形成以下'溶射層爽持構件之層 ① 底部塗覆物:80wt%Ni-20wt%Al δ〇 & ② 下部熔射絕緣層·· A 12 03 1 5 0 /z m m ③ 金屬質電極層:W50//m ④ 上部溶射絕緣層:之Al2〇3的15〇 “瓜 (2 )比較例的靜電失具構造 第16頁 2053-3738-PF.ptd 1240015 五、發明說明(14) ① 底部塗覆物:80wt%Ni-20wt%Al 80 vm ② 頂部塗覆物:88wt% Al203 - 1 2wt%Ti 02 300 //m 靜電吸附力是在〇·〇1 hpa的真空容器中,在矽晶圓 與靜電夾具負荷1分鐘的1KV電壓之後,將電源OFF,以測 定石夕晶圓從靜電夾具之脫離力(Pa)以進行測試。 其結果顯示,使用本發明之掙電夾具的話,在電源 0 F F之後吸附加立即消失,而比較例(習知技術)之 AI2 〇3 -T 1 Ο?構成的靜電夾具的話,直到吸附加消失需要 3 0〜4 5秒0 實施例4 在當作本發明靜電夾持構件層之鋁基材(寬度5 Omm X 長度50mm X厚度5mm)施以喷砂處理以粗面化之後,利用弧 光炼射法處理80wt%Ni—2〇wt%Al合金為7〇 的厚度。然 ,,利用電漿熔射法在上方形成厚度18〇 //111的人12〇3,接 f,利用電漿熔射法在上方形成5〇 V m的金屬鎢。其 次,利用電漿熔射法在上方形成厚度2〇〇 的^以,然後- 立=利用市售之液狀有機石夕樹脂,以當作封孔劑進行塗佈 乾燥’然後以此當作試驗片。 立、將式驗片的一定面積(l〇mjn><l〇mm)露出之後,其他 邛刀遮蓋起來’然後在含有鹵素化合物的氣體之中,電漿·· =電連、、、只4 0個小時,之後利用最大損失厚度以評估因電漿 腐蝕造成的損失量。 試驗條件1240015 V. Description of the invention (13) Table 2 Surface mi mi ~~ Thermal shock condition No. Bottom coating lower insulation layer metal electrode layer upper green insulation layer 350〇CX 15 minutes < = > Air cooling note 1 Yes Yes Yes * 0) No abnormality even after 10 cycles. Comparative Example 2 Yes Yes Yes * (2) No abnormality after 10 cycles 3 Yes No No No abnormality after 3 cycles 4 No No No Examples of non-abnormal inventions (Remarks) (1) The bottom coating is 80wt% Ni—20wt% A1 with a thickness of 100 // m. (2) The metal electrode layer * (1) is the atmospheric plasma spray method. Forming a metal w of 30 (the oxygen content is 0 · 丨 2 ^^ reference * (2) is a metal W forming a 30 r,. ^ ^ ^ By a reduced pressure plasma spray method (oxygen content of 0.12 wt%) (3) The insulating layer is a 1 〇. + 丄 ^ ΓWhite 1 The atmospheric spray method 150 β m using Ai 2 0 3 Example 3 This example is to attach a silicon wafer to an electrostatic clamp to hold a power source. After the change in the residual adsorption force at OFF with time, the test (1) formed the following 'solvent-emitting layer holding structure' on a statically formed Ai substrate having a diameter of 6 适合 suitable for the conditions of the present invention. Layer ① Bottom coating: 80wt% Ni-20wt% Al δ〇 & ② Lower shot-emitting insulation layer · A 12 03 1 5 0 / zmm ③ Metal electrode layer: W50 // m ④ Upper shot-emitting insulation layer : The Al2O3 15o "Melon (2) Comparative Example of the Electrostatic Lost Structure" Page 16 2053-3738-PF.ptd 1240015 V. Description of the Invention (14) ① Bottom Coating: 80wt% Ni-20wt% Al 80 vm ② Top coating: 88wt% Al203-1 2wt% Ti 02 300 // m The electrostatic adsorption force is 1KV voltage on silicon wafer and electrostatic fixture for 1 minute in a vacuum container of 0 · 〇1 hpa After that, the power was turned off to measure the detachment force (Pa) of the Shixi wafer from the electrostatic jig for testing. The results show that the use of the power-generating jig of the present invention causes the adsorption and disappearance immediately after 0 FF of the power source, and compared For example (known technology) of an AI2 〇3 -T 1 〇? Electrostatic clamp, it takes 30 to 4 5 seconds until the adsorption and disappearance. Example 4 In the aluminum substrate used as the electrostatic clamping member layer of the present invention (Width 5 Omm X Length 50mm X Thickness 5mm) After sandblasting to roughen, 80wt% Ni—2 〇wt% Al alloy has a thickness of 70. However, a person 1203 with a thickness of 18 // 111 is formed on the top by a plasma spray method, and then f is formed by 50% on the top by a plasma spray method. m of metal tungsten. Next, a plasma thickness of 200 Å is formed on the top by the plasma spray method, and then-Li = using a commercially available liquid organic stone resin to coat and dry as a sealant, and then use this as Test strip. After a certain area (10mjn > < 10mm) of the test piece is exposed, the other trowels are covered up. Then, in a gas containing a halogen compound, the plasma ·· = electric connection, ..., only After 40 hours, the maximum loss thickness was used to assess the amount of loss due to plasma corrosion. Test conditions
,體組成 CF4+ l〇〇ml+02 l〇ml + Ar 1 00 0 ml 高周波輸出1200W, Body composition CF4 + lOOml + 02 lml + Ar 10000 ml High frequency output 1200W
1240015 五、發明說明(15) ' -- 壓, 大氣壓 再者,此試驗的比較例係將A1基板經過Almite 後,形成與本發明相同的層構造,然後形成2〇〇 “ m1240015 V. Description of the invention (15) '-Pressure, atmospheric pressure. In addition, the comparative example of this test is that after passing A1 substrate through Almite, the same layer structure as that of the present invention is formed, and then 200 “m
Al2〇3_12wt%Ti〇2當作上部熔射絕緣層,在相同的條 進行試驗。 此試驗的結果可得知,相對於本發明之溶射絕緣 12〜15 左右的腐蝕,比較例的Almite處理薄層完全; 失,而基材之A1也損失(5〇〜7〇ym),並且Αΐ2〇3+η〇声 現3卜38 的損失,本發明之靜電夾持構件 2 ^ ·· 合物的電漿環境中極為安定。 頁S素化 產業上之利用可能性 如上所說明,本發明的靜電夾持構件除了耐衝 耐^性、耐磨耗性佳之外,由於金屬質溶射電極層的上 下精由Al2〇3陶瓷熔射絕緣層失持以形成三明治 ;庫倫力可固定石夕晶圓,所以去除電源時固持力U利 失,而使矽晶圓容易脫離,而可提昇作業效率。 2 電夾持構件的頂部塗覆物係 ,射塗覆薄層構成,所以對於與石夕晶圓接 .是電浆磨耗作用具有良好的抵抗力,不但能夠 ,層的微粉化’同時化學安定性高,所以亦抑制環境成份 效果並合且物成A等)的腐餘反應’而具有防止環境污染的 不直接眼-於之靜電夾持構件之金屬質熔射電極層Al2O3_12wt% Ti02 was used as the upper shot-fired insulating layer, and the test was performed on the same strip. The results of this test show that the Almite-treated thin layer of the comparative example is completely lost compared to the corrosion of the solvent-emission insulation of the present invention at about 12 to 15; and the substrate A1 is also lost (50 to 70 ym), and Αΐ203 + η〇 sounds the loss of 3 to 38, and the electrostatic clamping member 2 ^ ·· composition of the present invention is extremely stable in the plasma environment. As described above, in the chemical industry, the electrostatic clamping member of the present invention has excellent impact resistance and abrasion resistance. In addition, the upper and lower surfaces of the metal-soluble radiation electrode layer are melted by Al203 ceramics. The insulating layer is lost to form a sandwich; the Coulomb force can fix the Shi Xi wafer, so the holding force U is lost when the power is removed, and the silicon wafer is easily detached, which can improve the operating efficiency. 2 The top coating system of the electric clamping member is composed of a thin coating layer, so it is resistant to the abrasion of the plasma. It has a good resistance to the abrasion of the plasma. It has high properties, so it also suppresses the residual reaction of environmental component effects and the formation of A, etc.), and has an indirect eye to prevent environmental pollution-the metal ejection electrode layer of the electrostatic clamping member
間仍然月匕夠維持卓越的功能,有效率地促進石夕晶圓等電IIt is still enough to maintain excellent functions and effectively promote electric power such as Shi Xi wafers.
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- 2000-01-21 JP JP2000012818A patent/JP4272786B2/en not_active Expired - Lifetime
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- 2001-01-17 US US10/169,755 patent/US6771483B2/en not_active Expired - Lifetime
- 2001-01-17 KR KR10-2002-7009199A patent/KR100510572B1/en active IP Right Review Request
- 2001-01-17 EP EP01901396A patent/EP1258918B1/en not_active Expired - Lifetime
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KR20020070340A (en) | 2002-09-05 |
EP1258918B1 (en) | 2008-12-03 |
EP1258918A4 (en) | 2006-12-06 |
KR100510572B1 (en) | 2005-08-26 |
EP1258918A1 (en) | 2002-11-20 |
US6771483B2 (en) | 2004-08-03 |
DE60136793D1 (en) | 2009-01-15 |
JP2001203258A (en) | 2001-07-27 |
JP4272786B2 (en) | 2009-06-03 |
US20030007308A1 (en) | 2003-01-09 |
WO2001054188A1 (en) | 2001-07-26 |
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